HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 72545728, compound → HCID 72545729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 72545728 | HCID 72545728 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 72545729 | HCID 72545729 | 0.8% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
To a stirred solution of the crude material (22 mg) containing 6-bromo-5,7-dimethyl-4-(4-nitrophenyl)-2H-chromen-2-one (7-2) in EtOH (0.75 mL) and acetic acid (0.15 mL) was added iron (16 mg, 0.29 mmol) at room temperature. The mixture was heated at 110° C. for 2.5 h. The reaction mixture was then cooled at room temperature and filtrated. To the filtrate was added EtOAc and saturated NaHCO3 solution, and extracted with EtOAc. The organic layers were washed with brine, dried over Na2SO4 and concentrated. The residues was purified by silica gel column chromatography (hexane:EtOAc=5:1˜2:1) to give the title compound 7-3 (4.0 mg, 0.8% yield, 2 steps) as an orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09416121B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-2bdc589d930443d994e71d23e94b7789 |
| Source note | uspto-grants-2016_08 |